CN111298752A - Continuous production equipment for free radical polymerization and use method thereof - Google Patents
Continuous production equipment for free radical polymerization and use method thereof Download PDFInfo
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- CN111298752A CN111298752A CN202010289921.XA CN202010289921A CN111298752A CN 111298752 A CN111298752 A CN 111298752A CN 202010289921 A CN202010289921 A CN 202010289921A CN 111298752 A CN111298752 A CN 111298752A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/24—Stationary reactors without moving elements inside
- B01J19/2415—Tubular reactors
- B01J19/242—Tubular reactors in series
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/08—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
- B01J8/10—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles moved by stirrers or by rotary drums or rotary receptacles or endless belts
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/01—Processes of polymerisation characterised by special features of the polymerisation apparatus used
Abstract
The invention discloses continuous production equipment for free radical polymerization, which comprises tank reactors I and II and a tank reactor, wherein the top of the reactor I is connected with a monomer storage tank a, a monomer storage tank b, a catalyst storage tank and a polymerization inhibitor storage tank a, the top of the reactor II is connected with a polymerization inhibitor storage tank b, reaction pipes which are connected in series are distributed in the tank reactor, the first reaction pipe is connected with an initiator storage tank, the last reaction pipe is provided with a sampling port, a three-way valve of the reactor I is communicated with a feed inlet of the tank reactor, a discharge outlet of the tank reactor is communicated with the top of the reactor II, and the three-way valve of the reactor II is communicated with the top of the reactor I. The invention can ensure that the monomer and the catalyst are uniformly mixed in the reactor I, and the mixture enters the tank reactor and then is added with the initiator for reaction, can control the reaction temperature in a proper range, avoids the problem of over-concentrated reaction heat release in the tank reactor, and ensures that the reaction is more stable.
Description
Technical Field
The invention relates to chemical equipment, in particular to continuous production equipment for free radical polymerization and a using method thereof.
Background
Radical polymerization is an important polymerization mode, and the polymerization mechanism of most polymers belongs to radical polymerization. Radical polymerization is initiated by an initiator to generate radicals, and the polymerization is terminated by steps such as chain growth, chain termination and chain transfer. Wherein, a large amount of free radicals can be generated in the chain growth process, the molecular weight is sharply increased by the rapid reaction, the temperature of the system is obviously increased due to the exothermic reaction, and if no external control is available, the phenomenon of 'implosion' can occur, so that the material is agglomerated and scrapped. The free radical polymerization reaction is usually carried out in a reaction kettle, and in order to control the smooth progress of the polymerization, a batch polymerization mode is generally adopted, the production efficiency is relatively low, and the indexes of products in different batches are unstable.
Disclosure of Invention
Aiming at the characteristics of free radical polymerization, the invention provides continuous production equipment for free radical polymerization and a using method thereof, wherein the continuous production equipment is low in efficiency and unstable in product index by adopting an intermittent polymerization mode.
The technical scheme for solving the technical problems is as follows: a continuous production device for free radical polymerization comprises two tank-type reactors and two tank-type reactors, wherein the two tank-type reactors are respectively a reactor I and a reactor II, the top of the reactor I is connected with a monomer storage tank a, a monomer storage tank b, a catalyst storage tank and a polymerization inhibitor storage tank a, the top of the reactor II is connected with a polymerization inhibitor storage tank b, the tank bodies of the reactor I and the reactor II are both provided with circulating water heat-insulating jackets, and the bottoms of the reactor I and the reactor II are both provided with three-way valves; a plurality of reaction tubes connected in series are uniformly distributed in the tank reactor, the first reaction tube is connected with an initiator storage tank, the last reaction tube is provided with a sampling port, and the tank reactor is connected with a constant temperature water pump; one port of a three-way valve of the reactor I is communicated with a feed inlet of the groove type reactor through a circulating pump a, a discharge outlet of the groove type reactor is communicated with the top of the reactor II, and one port of the three-way valve of the reactor II is communicated with the top of the reactor I through a circulating pump b.
When the equipment is adopted to carry out free radical polymerization reaction, monomers and catalysts are uniformly mixed and heated in the reactor I, and the initiator is added after the mixture enters the tank reactor.
The tank reactor of the invention can adopt a conventional stirring type reaction kettle, and can also improve the prior reaction kettle as follows: the inside of tank reactor is equipped with scrapes wall formula agitator, scrapes wall formula agitator and includes motor, (mixing) shaft, crossbeam and wall scraping plate, and the motor setting is in tank reactor's top, (mixing) shaft links to each other with the pivot of motor, and the crossbeam vertical fixation is in on the (mixing) shaft, the wall scraping plate is fixed on the crossbeam, its one of which vertical edge with tank reactor's inner wall laminating.
Because the viscosity of the materials is gradually increased in the polymerization process, the materials can be attached to the inner wall of the reaction kettle, and the materials on the inner wall can be scraped by adopting the scraping wall type stirrer, so that the problems that the product performance is influenced by the attachment of the materials and the temperature control of the reaction kettle is possibly disabled are avoided.
Further, the wall scraping plate of the wall scraping stirrer is horizontally inclined by 30-60 degrees. The scraping plate inclines at a certain angle to generate vertical shearing force, so that the scraped materials can quickly enter the mixture.
In order to more effectively increase the temperature control of the reactants, the reaction tube may be formed in a spiral shape. The spiral reaction tube can prolong the running distance of reaction materials, can fully disperse heat, prevent the materials from implosion and enable free radical polymerization to be carried out more stably. According to the actual situation, better temperature control can be realized by selecting 2-6 reaction tubes.
Furthermore, uniform bulges can be arranged on the inner wall of the reaction tube, and the bulges are thread bulges, scale-shaped bulges or conical bulges. Set up the arch and can make the inhomogeneous flow of material, make the material mix more evenly, and do benefit to the heat dissipation. The bulges of each reaction tube are not limited by the types of the bulges of other reaction tubes and can be matched at will according to actual requirements.
The operation steps for realizing the continuous production of the free radical polymerization by adopting the equipment are as follows:
1) filling monomers, a catalyst, a polymerization inhibitor and an initiator into corresponding storage tanks, opening circulating water of a reactor I and a reactor II, and opening a constant temperature water pump of a tank reactor;
2) opening a monomer storage tank a and a monomer storage tank b, pumping different monomers with required dosage into a reactor I, opening a stirrer of the reactor I, opening a catalyst storage tank, adding a catalyst, and keeping stirring;
3) adjusting a three-way valve of the reactor I to be communicated with a feed inlet of a first reaction tube of the tank reactor, opening a circulating pump a, opening an initiator storage tank, and adding an initiator;
4) pumping the mixture into a reactor II, opening a stirrer of the reactor II, adjusting a three-way valve of the reactor II to be communicated with the top of the reactor I, and opening a circulating pump b to enable the mixture to circulate among the reactor I, the reactor II and a tank reactor;
5) sampling at a sampling port, and opening an initiator storage tank according to the reaction degree of the sample to add the initiator;
6) when sampling detection shows that the polymerization degree reaches the standard, opening a polymerization inhibitor storage tank a and a polymerization inhibitor storage tank b at the same time, adding a polymerization inhibitor, circulating for a period of time, adjusting one of three-way valves, and leading out reactants;
7) and (5) repeating the steps 1) to 6) to realize continuous production.
Drawings
FIG. 1 is a schematic diagram of the apparatus of the present invention; FIG. 2 is a cross-sectional view of a tank reactor; FIG. 3 is a sectional view of a reaction tube with thread-like projections; FIG. 4 is a sectional view of a scale-like projection reaction tube; FIG. 5 is a sectional view of a reaction tube with a conical projection; each part is as follows:
1. the reactor comprises a reactor I, 1-1, a monomer storage tank a, 1-2, a monomer storage tank b, 1-3, a catalyst storage tank, 1-4, a polymerization inhibitor storage tank a, 1-5, a circulating pump a, 2, a reactor II, 2-1, a polymerization inhibitor storage tank b, 2-2, a circulating pump b, 3, a groove type reactor, 4, a reaction tube, 4-1, a thread-shaped bulge, 4-2, a scale-shaped bulge, 4-3, a conical bulge, 5, an initiator storage tank, 6, a sampling port, 7, a constant temperature water pump, 8, a stirring shaft, 9, a cross beam, 10 and a scraping wall plate.
Detailed Description
The present invention is described below with reference to examples, which are provided for illustration only and are not intended to limit the scope of the present invention.
Example 1
As shown in figure 1, the continuous production equipment for free radical polymerization comprises two tank reactors, namely a reactor I1 and a reactor II 2, wherein the top of the reactor I1 is connected with a monomer storage tank a1-1, a monomer storage tank b1-2, a catalyst storage tank 1-3 and a polymerization inhibitor storage tank a1-4, the top of the reactor II 2 is connected with a polymerization inhibitor storage tank b2-1, the reactor I1 and the reactor II 2 are both provided with circulating water heat-preservation jackets, and the bottoms of the reactor I1 and the reactor II 2 are both provided with three-way valves; 2 reaction tubes 4 which are connected in series are uniformly distributed in the tank reactor 3, an initiator storage tank 5 is connected to the first reaction tube 4, a sampling port 6 is arranged on the last reaction tube 4, and the tank reactor 3 is connected with a constant temperature water pump 7; one port of a three-way valve of the reactor I1 is communicated with a feed inlet of the tank reactor 3 through a circulating pump a1-5, a discharge outlet of the tank reactor 3 is communicated with the top of the reactor II 2, and one port of a three-way valve of the reactor II 2 is communicated with the top of the reactor I1 through a circulating pump b 2-2.
Example 2
Referring to fig. 1 and 2, a continuous production device for free radical polymerization comprises two tank reactors, namely a reactor I1 and a reactor II 2, wherein the top of the reactor I1 is connected with a monomer storage tank a1-1, a monomer storage tank b1-2, a catalyst storage tank 1-3 and a polymerization inhibitor storage tank a1-4, the top of the reactor II 2 is connected with a polymerization inhibitor storage tank b2-1, the reactor I1 and the reactor II 2 are both provided with circulating water heat-preservation jackets, and the bottoms of the reactor I1 and the reactor II 2 are both provided with three-way valves; wall scraping stirrers are arranged in the reactor I1 and the reactor II 2 respectively, each wall scraping stirrer comprises a motor, a stirring shaft 8, a cross beam 9 and a wall scraping plate 10, the motors are arranged at the top of the tank reactor, the stirring shafts 8 are connected with rotating shafts of the motors, the cross beams 9 are vertically fixed on the stirring shafts 8, the wall scraping plates 10 are fixed on the cross beams 9 and horizontally inclined by 45 degrees, and one vertical edge of each wall scraping stirrer is attached to the inner wall of the tank reactor; 6 reaction tubes 4 which are connected in series are uniformly distributed in the tank reactor 3, an initiator storage tank 5 is connected to the first reaction tube 4, a sampling port 6 is arranged on the last reaction tube 4, and the tank reactor 3 is connected with a constant temperature water pump 7; one port of a three-way valve of the reactor I1 is communicated with a feed inlet of the tank reactor 3 through a circulating pump a1-5, a discharge outlet of the tank reactor 3 is communicated with the top of the reactor II 2, and one port of a three-way valve of the reactor II 2 is communicated with the top of the reactor I1 through a circulating pump b 2-2.
Example 3
Referring to FIGS. 1-5, a continuous production apparatus for radical polymerization comprises two tank reactors, namely a reactor I1 and a reactor II 2, wherein the top of the reactor I1 is connected with a monomer storage tank a1-1, a monomer storage tank b1-2, a catalyst storage tank 1-3 and a polymerization inhibitor storage tank a1-4, the top of the reactor II 2 is connected with a polymerization inhibitor storage tank b2-1, the reactor I1 and the reactor II 2 are both provided with circulating water heat-preservation jackets, and the bottoms of the reactor I1 and the reactor II 2 are both provided with three-way valves; wall scraping stirrers are arranged in the reactor I1 and the reactor II 2 respectively, each wall scraping stirrer comprises a motor, a stirring shaft 8, a cross beam 9 and a wall scraping plate 10, the motors are arranged at the top of the tank reactor, the stirring shafts 8 are connected with rotating shafts of the motors, the cross beams 9 are vertically fixed on the stirring shafts 8, the wall scraping plates 10 are fixed on the cross beams 9 and horizontally inclined by 45 degrees, and one vertical edge of each wall scraping stirrer is attached to the inner wall of the tank reactor; 3 reaction tubes 4 which are connected in series are uniformly distributed in the tank reactor 3, the reaction tubes 4 are spiral, uniform thread-shaped bulges 4-1 are arranged on the inner wall of the first reaction tube 4, uniform scale-shaped bulges 4-2 are arranged on the inner wall of the second reaction tube 4, uniform conical bulges 4-3 are arranged on the inner wall of the third reaction tube 4, an initiator storage tank 5 is connected on the first reaction tube 4, a sampling port 6 is arranged on the last reaction tube 4, and the tank reactor 3 is connected with a constant temperature water pump 7; one port of a three-way valve of the reactor I1 is communicated with a feed inlet of the tank reactor 3 through a circulating pump a1-5, a discharge outlet of the tank reactor 3 is communicated with the top of the reactor II 2, and one port of a three-way valve of the reactor II 2 is communicated with the top of the reactor I1 through a circulating pump b 2-2.
The equipment of example 3 is adopted to carry out the free radical polymerization reaction of the modified silica aerogel and methacrylic acid, and the steps are as follows:
1) raw material preparation
Adding 1000 parts by weight of coupling agent KH550 into a glass beaker, stirring at 180rpm, adding 100 parts by weight of silicon dioxide aerogel, controlling the temperature at 45 ℃, stirring for 3 hours, transferring into an ultrasonic oscillator under the protection of nitrogen, ultrasonically dispersing for 3 hours, standing for 12 hours, vacuum-filtering, and vacuum-drying a filter cake for 6 hours at 75 ℃ to obtain powder for later use; adding 1000 parts by weight of formamide into a three-neck glass flask, carrying out water bath at 45 ℃, keeping stirring, adding 120 parts by weight of the obtained powder, controlling the stirring speed to be 80rpm, reacting at 50 ℃ for 4 hours to obtain formamide modified nano-silica aerogel, transferring 120kg of product into a monomer storage tank a, and keeping stirring; adding 1500kg of methacrylic acid into a monomer storage tank b, adding 6kg of initiator azodiisobutyronitrile into an initiator storage tank, and adding 5kg of polymerization inhibitor tetrachlorobenzoquinone into a polymerization inhibitor storage tank a and a polymerization inhibitor storage tank b respectively;
2) mixing
Opening circulating water heat-preservation jackets of the reactor I and the reactor II, controlling the temperature of the circulating water to be 25 ℃, opening a monomer storage tank, pumping methacrylic acid into the reactor I, opening a wall scraping type stirrer, opening a monomer storage tank a, uniformly dividing formamide modified nano-silica aerogel for 6 times, pumping the formamide modified nano-silica aerogel into the reactor I, adjusting the stirring speed to 180rpm, and stirring for 6 hours;
3) cyclic reaction
Opening a constant temperature water pump, adjusting the temperature to 40 ℃, opening a circulating pump a1-5 and a circulating pump b2-2, pumping the mixture into a tank reactor, opening a valve of an initiator storage tank, adding part of the initiator, carrying out cyclic reaction for 8 hours, sampling from a sampling port every 1 hour, detecting the viscosity of the mixture, adding the rest of the initiator into the system in several times, simultaneously opening a polymerization inhibitor storage tank a and a polymerization inhibitor storage tank b, adding a polymerization inhibitor, and carrying out recycling for 2 hours, wherein in the cyclic process, corresponding materials are respectively filled into the monomer storage tank a, the monomer storage tank b, the initiator storage tank, the polymerization inhibitor storage tank a and the polymerization inhibitor storage tank b according to the weight of the step 1);
4) continuous production
Adjusting a three-way valve of the reactor I or the reactor II, discharging reaction materials in the system, and then repeating the operations of the steps 2) and 3) to realize continuous production.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (7)
1. A continuous production device for free radical polymerization comprises two tank-type reactors and two tank-type reactors, and is characterized in that the two tank-type reactors are respectively a reactor I and a reactor II, the top of the reactor I is connected with a monomer storage tank a, a monomer storage tank b, a catalyst storage tank and a polymerization inhibitor storage tank a, the top of the reactor II is connected with a polymerization inhibitor storage tank b, the tank bodies of the reactor I and the reactor II are both provided with circulating water heat-preservation jackets, and the bottoms of the reactor I and the reactor II are both provided with three-way valves;
a plurality of reaction tubes connected in series are uniformly distributed in the tank reactor, the first reaction tube is connected with an initiator storage tank, the last reaction tube is provided with a sampling port, and the tank reactor is connected with a constant temperature water pump;
one port of a three-way valve of the reactor I is communicated with a feed inlet of the tank reactor through a circulating pump a, a discharge outlet of the tank reactor is communicated with the top of the reactor II, and one port of a three-way valve of the reactor II is communicated with the top of the reactor I through a circulating pump b.
2. The continuous production apparatus for radical polymerization according to claim 1, wherein a wall scraping stirrer is disposed inside the tank reactor, the wall scraping stirrer comprises a motor, a stirring shaft, a cross beam and a wall scraping plate, the motor is disposed at the top of the tank reactor, the stirring shaft is connected with a rotating shaft of the motor, the cross beam is vertically fixed on the stirring shaft, the wall scraping plate is fixed on the cross beam, and a vertical edge of the wall scraping plate is attached to the inner wall of the tank reactor.
3. The continuous production apparatus for radical polymerization according to claim 2, wherein the wall scraping plate is horizontally inclined at 30 ° to 60 °.
4. The continuous production apparatus for radical polymerization according to claim 1, wherein the reaction tube has a spiral shape.
5. The continuous production apparatus for radical polymerization according to claim 4, wherein the number of reaction tubes is 2 to 6.
6. The continuous production apparatus for radical polymerization according to claim 5, wherein the inner wall of the reaction tube is provided with uniform protrusions, the protrusions are screw-shaped protrusions, scale-shaped protrusions or tapered protrusions, and the reaction tube is independently selected from any one of the protrusions.
7. A continuous production process for radical polymerization, characterized in that use is made of a device according to any one of claims 1 to 6, comprising the following steps:
1) filling monomers, a catalyst, a polymerization inhibitor and an initiator into corresponding storage tanks, opening circulating water of a reactor I and a reactor II, and opening a constant temperature water pump of a tank reactor;
2) opening a monomer storage tank a and a monomer storage tank b, pumping different monomers with required dosage into a reactor I, opening a stirrer of the reactor I, opening a catalyst storage tank, adding a catalyst, and keeping stirring;
3) adjusting a three-way valve of the reactor I to be communicated with a feed inlet of a first reaction tube of the tank reactor, opening a circulating pump a, opening an initiator storage tank, and adding an initiator;
4) pumping the mixture into a reactor II, opening a stirrer of the reactor II, adjusting a three-way valve of the reactor II to be communicated with the top of the reactor I, and opening a circulating pump b to enable the mixture to circulate among the reactor I, the reactor II and a tank reactor;
5) sampling at a sampling port, and opening an initiator storage tank according to the reaction degree of the sample to add the initiator;
6) when sampling detection shows that the polymerization degree reaches the standard, opening a polymerization inhibitor storage tank a and a polymerization inhibitor storage tank b at the same time, adding a polymerization inhibitor, circulating for a period of time, adjusting one of three-way valves, and leading out reactants;
7) and (5) repeating the steps 1) to 6) to realize continuous production.
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| CN202010289921.XA CN111298752A (en) | 2020-04-14 | 2020-04-14 | Continuous production equipment for free radical polymerization and use method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112552359A (en) * | 2020-12-21 | 2021-03-26 | 北京大学 | Automatic preparation method of fondaparinux sodium pentasaccharide intermediate |
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- 2020-04-14 CN CN202010289921.XA patent/CN111298752A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112552359A (en) * | 2020-12-21 | 2021-03-26 | 北京大学 | Automatic preparation method of fondaparinux sodium pentasaccharide intermediate |
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